CN111943264A - Preparation method and application of gilding nano flaky material with excellent photoelectric property - Google Patents
Preparation method and application of gilding nano flaky material with excellent photoelectric property Download PDFInfo
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- 238000000034 method Methods 0.000 claims abstract description 9
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- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- 239000002135 nanosheet Substances 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004809 Teflon Substances 0.000 claims description 5
- 229920006362 Teflon® Polymers 0.000 claims description 5
- 239000002064 nanoplatelet Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 230000005693 optoelectronics Effects 0.000 claims 5
- 238000001816 cooling Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
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- 238000007747 plating Methods 0.000 description 3
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- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
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- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
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- 241001330002 Bambuseae Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- DDNCQMVWWZOMLN-IRLDBZIGSA-N Vinpocetine Chemical compound C1=CC=C2C(CCN3CCC4)=C5[C@@H]3[C@]4(CC)C=C(C(=O)OCC)N5C2=C1 DDNCQMVWWZOMLN-IRLDBZIGSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- 239000012153 distilled water Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229960000744 vinpocetine Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/40—Electric properties
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention relates to a gilding nano flaky material with excellent photoelectric property, belonging to the technical field of inorganic nano materials. The invention synthesizes gilded Bi with excellent photoelectric property9O7.5S6The method is simple and easy to operate, conditions are easy to control, and the obtained material is novel in appearance and has excellent photoelectric properties. Provides a simple and convenient way for synthesizing bismuth-based nano materials with excellent photoelectric properties in the future, and can be applied to the field of photoelectric devices on a large scale.
Description
Technical Field
The invention relates to a gilding nano flaky material with excellent photoelectric property, belonging to the technical field of inorganic nano materials.
Background
Bi9O7.5S6Is provided with a space group
The absorption band edge of the semiconductor with the rhombohedron structure and the direct band gap is 940nm and is positioned in a near infrared region, so that the semiconductor has good absorption on visible light and has application potential in the construction of photovoltaic equipment. On a macroscopic scale, Bi9O7.5S6Gold platingThe phenomenon of (1) is shown in fig. 1, at present, perfume, skin care products and the like with the gold-plating phenomenon appear to improve the aesthetic feeling of the products, the phenomenon of gold-plating is valuable for research, and in addition, gold-plating materials can be used as coatings to enable the products to have artistic feeling. Microscopically, Bi9O7.5S6Has a unique layered structure and is characterized by [ BiS2]And [ Bi ]2O2]Layer edge [001]The directions are alternately stacked. In addition, Bi9O7.5S6The compound has the advantages of low cost, no toxicity, simple operation and the like, and becomes an ideal choice for the photoelectric detector. In 2015, Huangfuqiang et al (Meng, Zhang et al 2015) successfully synthesized a novel layered compound Bi for the first time by a simple hydrothermal method9O7.5S6Nanosheets, and their resistivity was found to be temperature dependent by Variable Range Hopping (VRH) and adiabatic Small Polaron Hopping (SPH) test results, confirming the semiconducting properties of the compound. In conclusion, for Bi9O7.5S6The research on the performance of the nano-sheet is very necessary, such as photoelectric performance and the like. The invention has the same thiourea as the thiourea for providing the sulfur source, and the other raw materials are different, and the raw materials for regulating and controlling the pH value are simpler and better to operate, the reaction temperature is lower than that of the raw materials, the reaction time is short, and the operation is simple.
Researchers have now developed a method of synthesizing this material (Meng, Zhang et al.2015): 0.01mol of Bi (NO)3·5H2O，0.01mol SC(NH2)25g of KOH and 10g of LiOH were dissolved in 10ml of a NaCl mixed solution. Distilled water and alcohol (volume ratio 1: 1) were continuously stirred. The precursor was then transferred to a 50mL stainless steel autoclave lined with polytetrafluoroethylene to achieve a 75% fill. The crystal reacts for 72 hours at 180 ℃, and finally the single crystal Bi is successfully synthesized9O7.5S6Of (4) a dark powder. The resulting morphology is shown in FIG. 5. However, the thickness of the material combined in this subject is about 6 μm, and the optical responsivity is low, and the thickness of the material combined in this subject is small and the photoelectric properties are excellent as compared with the material combined in this subject.
Disclosure of Invention
The invention isThe technical problem solved is that: provides a preparation method of gilding nano flaky material with excellent photoelectric property, and obtains a Bi gilding material with excellent photoelectric property by a solvothermal method9O7.5S6The preparation method of the nanosheet material is simple and easy to operate, is environment-friendly, and shows excellent photoelectric response under the irradiation of laser with different intensities and different wavelengths, so that the nanosheet material has wide application prospects in the fields of photoelectric devices, solar cells and the like.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the method adopted by the invention is as follows: adopts a solvothermal method to synthesize gilded Bi with excellent photoelectric property9O7.5S6The nano-sheet material is uniform, has good dispersibility and high yield which can reach 75 percent. The method has the advantages of simple preparation conditions, simplicity, easy obtaining and high repeatability.
The invention has the beneficial effects that:
compared with novel bamboo leaf-shaped bismuth sulfide (2020100203660), Bi9O7.5S6The synthesis step of the nano flaky material is sodium hydroxide aqueous solution with pH adjusted, and the reaction condition of the bismuth sulfide of the invention is sodium hydroxide glycol solution with pH adjusted.
In addition, gilded Bi with excellent photoelectric properties9O7.5S6The nano flaky material has excellent photoelectric response characteristics and can be applied to the field of photoelectric response devices.
The invention synthesizes gilded Bi with excellent photoelectric property9O7.5S6The method is simple and easy to operate, conditions are easy to control, and the obtained material is novel in appearance and has excellent photoelectric properties.
Provides a simple and convenient way for synthesizing bismuth-based nano materials with excellent photoelectric properties in the future, and can be applied to the field of photoelectric devices on a large scale.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 shows a macroscopic view of Bi with gilding phenomenon9O7.5S6A picture of the material.
FIG. 2 shows (a, b) gilded Bi with excellent photoelectric properties9O7.5S6The appearance characterization of the nano flaky material under a field emission scanning electron microscope (c) gilded Bi with excellent photoelectric property9O7.5S6And (3) characterizing the appearance of the nano sheet material under a transmission electron microscope.
FIG. 3 shows gilded Bi with excellent photoelectric properties9O7.5S6XRD pattern of nanoplatelets.
FIG. 4 shows gilded Bi9O7.5S6The photoelectric performance test result of the nano sheet material; (a) current-voltage (I-V) curves at white light with different powers; (b) current-time (I-t) curves at white light with different powers; (c) the relationship curve of photocurrent and illumination intensity; (d) current-voltage (I-V) curves at lasers with different wavelengths; (e) current-time (I-t) curves under lasers with different wavelengths; (f) a histogram of photocurrent versus wavelength.
FIG. 5 shows Bi having the same crystal structure9O7.5S6Nanosheets.
Detailed Description
Example 1
Gilded Bi with excellent photoelectric property9O7.5S6The preparation steps of the nano flaky material are as follows:
in a typical synthesis, 0.025mmol of bismuth chloride (BiCl)3) 0.690mmol polyvinylpyrrolidone (PVP) and 0.386mmol thiourea (CH)4N2S) was dissolved in 7mL of Ethylene Glycol (EG), and then 778 μ L of an aqueous NaOH (1M) solution was added to the above mixture for pH adjustment (pH 13). Finally, the precursor solution was transferred to a teflon lined stainless steel autoclave (10% fill) and held at 150 ℃ for 3 hours. After the autoclave had been cooled naturally to room temperature, the product was centrifuged and washed 3 times with a mixture of acetone and water (1: 1), thenThe samples were then freeze dried for 24 h. Finally, Bi is obtained9O7.5S6A nano-platelet material. Adding 2 mu L of Bi9O7.5S6The solution was dropped onto a silicon wafer which had been cleaned, naturally dried, and then Bi was characterized using a JEOL JSM-7600F field emission scanning electron microscope (FE-SEM) at an acceleration voltage of 3kV and using a JEOL 2100Plus Transmission Electron Microscope (TEM) at an acceleration voltage of 200kV9O7.5S6The morphology of the sheet material is shown in FIGS. 2 (a-c).
Of note in the above steps are:
1. the filling degree of the reaction can be adjusted to 10 percent, 50 percent, 70 percent and 95 percent, and the gilded Bi with excellent photoelectric property can be directly obtained9O7.5S6A nano-sheet material; among them, the packing degree is preferably 10% and the yield is the highest.
2. Bismuth chloride can be controlled to be 1.40-69mg/mL, polyvinylpyrrolidone can be controlled to be 11.1-555mg/mL, thiourea can be controlled to be 0.4-21mg/mL, and the volume of ethylene glycol can be controlled to be 1-100mL, so that Bi can be obtained9O7.5S6A nanosheet material;
3. the reaction temperature can be regulated to between 110-200 ℃ to obtain Bi9O7.5S6A nanosheet material.
The brown powder obtained after freeze-drying (obtained with a filling degree of 10%) was characterized by X-ray diffraction (XRD) and Bi was found9O7.5S6The sheet material corresponded to PDF card (JCPDS NO.1520006) and was free of miscellaneous peaks, as shown in FIG. 3.
Note: x-ray diffraction (XRD) characterization on SmartLab (Rigaku) with Cu Ka1(k 0.154178nm) as light source for 4min-1To confirm the phase structure and purity of the crystals.
Gilded Bi9O7.5S6The application of the nano flaky material in the aspect of photoelectric devices:
and (3) photoelectric response test: 2mg of the freeze-dried product was dispersed in 500. mu.L of water, and then 20. mu.L of Bi was added9O7.5S6The solution was uniformly droppedOn the interdigital electrode (the area of the interdigital electrode is 2 × 1 cm)2And a spacing d of 0.1mm, mega bory scientific co., vinpocetine), and air-dried, and then the electrode was annealed at 350 c for 1h (in order to obtain Bi)9O7.5S6The membrane is firmly fixed to the interdigital electrodes), and naturally cooled. Next, Bi was tested on a function generator (AFG1022, Tektronix) with a two-electrode system9O7.5S6The photovoltaic properties of the film. At 5V and white light with different power (light intensity ranging from 0 to 315W/m)2) And Bi was measured under a laser having a different wavelength (wavelength ranging from 400nm to 760nm, power of 10mW)9O7.5S6And a current-voltage (I-V) curve tested under the white light and laser irradiation and a voltage in the range of-5V to 5V described above.
As shown in FIG. 4a, at 0 to 315W/m2The photocurrent of the material under white light illumination in the intensity range increased with increasing optical power intensity, which is consistent with the fact that the photogeneration efficiency of the charge carriers is proportional to the absorbed photon flux, and the photocurrent still appeared very stable, indicating that Bi9O7.5S6The photoelectric response of the nano-sheet has excellent stability. As shown in fig. 4b, by periodically switching the light source on and off at a bias of 5V, no significant attenuation of the intensity of the two currents (photocurrent and dark current) can be observed, and the photocurrent state is relatively stable, indicating good stability and repeatability of the material. As shown in fig. 4c, there is a power function relationship between the photocurrent and the corresponding light irradiance. As one of the key parameters for evaluating the response efficiency of the detector to the light signal, the responsivity (R) can be calculated as follows:
wherein, IlightIs the current measured under irradiation, P is the power intensity of the light impinging on the photodetector, E is the optical power density, and S is the photosensitive area of the photodetector. According to the formula, the radiation intensity is calculated to be 5-315W/m2In the range of 315W/m of irradiation intensity2Under the irradiation of light, the R value of the photoelectric device is 3.50mA W-1. As shown in FIG. 4d-f, Bi was irradiated with a laser beam having a wavelength ranging from 400nm to 760nm (incident power of about 20 mW)9O7.5S6The nanosheet is excellent in photoelectric response in the shallow ultraviolet region and exhibits stable photoelectric response performance.
Therefore, Bi is excellent in light of the good photoresponse characteristics9O7.5S6The nanosheets are a good choice for photosensitive switch applications.
Example 2
Example 2 is essentially the same as example 1, except that: in a typical synthesis, 0.05 mmol of bismuth chloride (BiCl)3) 1.38mmol of polyvinylpyrrolidone (PVP) and 0.77mmol of thiourea (CH)4N2S) was dissolved in 14mL of Ethylene Glycol (EG), and then 778 μ L of an aqueous NaOH (1M) solution was added to the above mixture for pH adjustment (pH 13). Finally, the precursor solution was transferred to a teflon lined stainless steel autoclave (50% fill) and held at 150 ℃ for 3 hours. After the autoclave was naturally cooled to room temperature, the product was centrifuged and washed 3 times with a mixture of acetone and water (1: 1), and then the sample was freeze-dried for 24 h. Finally, Bi is obtained9O7.5S6A nano-platelet material.
The invention is not limited to the specific technical solutions described in the above embodiments, and all technical solutions formed by equivalent substitutions are within the scope of the invention as claimed.
Claims (6)
1. A preparation method of gilding nano flaky material with excellent photoelectric property is characterized in that: adding bismuth chloride (BiCl)3) Polyvinylpyrrolidone (PVP) and thiourea (CH)4N2S) in Ethylene Glycol (EG), bismuth chloride at 1.40-69mg/mL, polyvinylpyrrolidone at 11.1-555mg/mL and thiourea at 0.4-21mg/mL, the volume of ethylene glycol at 1-100mL, then an aqueous NaOH solution was added to the mixture to adjust the pH (pH 13), the precursor solution was transferred to a Teflon lined stainless steel autoclave, 10-95% of which was placed in a Teflon lined stainless steel autoclaveFilling degree, reacting at 110-200 ℃ for 3-24 hours, naturally cooling the autoclave to room temperature, centrifuging the product, washing with a mixture of acetone and water for several times, freeze-drying the sample, and finally obtaining Bi9O7.5S6A nano-platelet material.
2. The method for preparing gilded nanosheet material having excellent optoelectronic properties as set forth in claim 1, wherein: wherein bismuth chloride is controlled to be 1.40mg/mL, polyvinylpyrrolidone is controlled to be 11.1mg/mL, and thiourea is controlled to be 1.70 mg/mL.
3. The method for preparing gilded nanosheet material having excellent optoelectronic properties as set forth in claim 1, wherein: 0.025mmol of bismuth chloride (BiCl)3) 0.690mmol polyvinylpyrrolidone (PVP) and 0.386mmol thiourea (CH)4N2S) was dissolved in 7mL of Ethylene Glycol (EG), then 778 μ L of aqueous NaOH (1M) solution was added to the above mixture for pH adjustment (pH 13), and finally the precursor solution was transferred to a teflon lined stainless steel autoclave (10% filling degree) and kept at 150 ℃ for 3 hours. After the autoclave was naturally cooled to room temperature, the product was centrifuged and washed 3 times with a mixture of acetone and water (1: 1), and then the sample was freeze-dried for 24 h. Finally, Bi is obtained9O7.5S6A nano-platelet material.
4. The method for preparing gilded nanosheet material having excellent optoelectronic properties as set forth in claim 1, wherein: the mixture is mixed with 2 mu L of Bi9O7.5S6The solution was dropped onto a silicon wafer which had been cleaned, naturally dried, and then bamboo-leaf-shaped Bi was characterized by using a JEOL JSM-7600F field emission scanning electron microscope (FE-SEM) at an acceleration voltage of 3kV and a JEOL 2100Plus Transmission Electron Microscope (TEM) at an acceleration voltage of 200kV2S3Morphology of the sheet material.
5. The gold-plated nano-sheet material obtained by the method for preparing gold-plated nano-sheet material with excellent photoelectric properties according to claims 1-4.
6. The application of the gilded nanosheet material with excellent optoelectronic properties of claim 5 in the fields of optoelectronic devices and solar cells.
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| CN111185196A (en) * | 2020-01-09 | 2020-05-22 | 南京工业大学 | Bamboo-leaf-shaped bismuth sulfide nano-sheet catalytic material and preparation method and application thereof |
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